Process of and apparatus for distilling and desulphurizing hydrocarbon oil



Patented Nov. 26, 1889'.

F. W. MINSHALL.

HYDROUARBON OIL.

$4 772 M flfimiml N. PETERS. PholwLiihogr-aphei. Washinglon. D.C.

(No Model.)

PROGESS OF AND APPARATUS FOR DISTILLING AND DBSULPHURIZI'NG UNITED STATES PATENT OEEIcE.

FRANK \V. MINSIIAIAIJ, OF MARIETTA, OllIO.

PROCESS OF AND APPARATUS FOR DISTILLING AND DESULPHURIZING HYDROCARBON OIL.

SPECIFICATION forming part of Letters Patent No. 415,876, dated November 26, 1889.

Application filed August 8, 1889. Serial No. 320,091. (No model.)

To all whom it may concern.-

citizen of the United States, residing at Marietta, in the county of \Vashington and State of Ohio, have invented a new and useful Improvement in the Process of and Apparatus for Distilling and Desulphurizing Hydrocarbon Oil, of which the following is a specification.

My invention relates to an improvement whereby the heavier or crude hydrocarbon oils may by a continuous or uninterrupted process be distilled and at the same time relieved of sulphur to render the distillate devoid of any sulphurous constituent; and I accomplish the object of my invention, broadly stated, by injecting hydrocarbon oil to be distilled and desulphurized with superheated steam and oxygen into a retort. and automatically maintaining a constantor substantially constant temperature inside the retort.

The apparatus for the practice of my improved process is illustrated in Figure 1 of the accompanying drawings in elevation, partly broken, and sectional; and Fig. 2 shows by an enlarged view in sectional elevation the pressure-regulating valve used with the apparatus.

A is an ordinary cylinder still or retort, supported over a suitable furnace B, having a fire-chan'iber r and the common appurtenances thereto, and C is the condenser, communieating through a conduit q with the retort near the rear end of the latter, and also communicating therewith through a pipe q, extending into the retort near its base. The pipes q and q serve, respectively, to conduct the vapors and residuum (tar) of distillation into the condenser, all in a usual manner, the parts thus far described corresponding with those in common use for distilling hydrocarbon oils.

Inside and lengthwise-of the retort A, near its base, is a thermostat D, comprising a brass rod 19, preferably about three-fourths of an inch in diameter, inside an extra-heavy iron pipe p, of a diameter to admit the rod 1; without binding, and supported at one end in the forward head of the retort-cylinder and adj acent wall and toward its opposite end, which is closed with a plug 12 having a central threaded socket, as shown, by a suitable leg Be it known that I, FRANK \V. MINsHALL,a

19 The rod 1:) is screwed at one end into the socket of the plug p and extends thence through the pipe 1) and through a stuffingbox 12 provided in its outer end, and in which I the brass rod works freely when expanded or contracted by the temperature within the retort beyond the forward end of the retortcylinder.

E is a steam-boiler adjacent to the retort, and between the two is a small steanrchest F, suitably and lirmly supported, as indicated, and having in its upper side ports 00 and 9;, into which lead, respectively, a pipe 0, communicatin g through a branch pipe 0' with'the steam-dome of the boiler, and a pipe a, communicating at its end, controllably, with the outer air, and between its extremities, through a pipe a, with one end of a superheater-coil G in the fire-chamber 0', the opposite end of the coil G leading into the pipe 0. In the steam-chest F is a piston-valve F, actuated from a valve-rod m, extending through an end of the steam-chest and through a suitable stuffing-box m, and pivotally connected with an end of a lever l-l, fulcrumed between its extremities, as shown at 1 and pivoted at its opposite end to the projecting end of the thermostat-rod 13.

On the under side of the steam-chest F are ports 06 and 1: coinciding, respectively, with the ports at and 42:, and with both of which communicates a pipe Zthrough two branches Z and Z The pipe Z leads from the aforesaid branches into a box or chamber is, opening at one end into the retort A, and communicating from its opposite end through a pipe '23, having a valve '21, with the oil-supply reservoir 1, near the base of the latter, and from which an overflow-pipe i leads to a suitable receptacle 1. with a valve It, leads from the pipe Z into a box or chamber 70, like the box is, opening into the retort-cylinder, and communicating at its outer end through a pipe g, provided with a-valve g, with the outer air or other supply of oxygen, and a thermometer K, the measuring capacity of which should reach as high as 650 Fahrenheit, is provided in the pipe 72 In the pipe Z, I provide a pressureregulating valve L and in the conduit q an ordinary spring check-valve e, and the pipes A branch pipe h, provided I 5 f therein.

0, 71, Z, and q should be provided with suitable valves, as indicated, to control the passages through them.

Y To practice my' improved process I first introduce into the retort A a quantity of hydrocarbon oil of so limwlity that it will require a temperature above 500 Fahrenheit to boil it, the quantity introduced being sufficient to cover the pipe 1) of the thermostat D. Fire is then started in the chamber 7 and the oil in the retort heated to 500 Fahrenheit, and steam is introduced from the boiler E into the superheater-coil G by closing the valve f in the pipe 0 and opening the valve The valve in the pipe 0 and the valve f in the pipe n are left open to allow the superheating steam to blow off until its temperature reaches 500 Fahrenheit, when the blow-off is closed and the valve f in the pipe n opened to permit the superheated steam to enter the chest F through the port :20, and thence by way of the pipe Z from the port 00 into. the retort through the box 7c. The spring of the check-valve din the conduit q is so adjusted as to make sufficient 45 for superheated steam.

back-pressure to .maintain the retort A filled with the superheated steam. Vith the introduction of superheated steam into the retort A the valve 1" in the oil-supply pipe t' and the valve g, controlling communication of the box 76 with the open air, (or with another supply of oxygen,) are opened, the fire in the chamber r' being continued to generate the heat required. Thus the hydrocarbon oil to be treated is subjected continuously to a temperature maintained constantly at about 500 Fahrenheit by the automatic action of the thermostat, which is as follows: The initial adjustment of the 40 valve F in the steam-chest F is such that from the boiler E, whereby entrance of such common or wet steam into the retort is permitted and produces lowering of the temperature, which, when it becomes reduced below that stated, actuates the valve F by contraction of the rod p to admit more superheated steam and less or no steam from the boiler.

The oil placed in the retort A, which should be of greater specific gravity than that in the receptacle I, aids in maintaining constant the temperature inside the retort, since, because it boils at a certain temperature (as 500 Fahrenheit) and is continuously supplied with heat from the furnace and with super- 6 5 heated steam at a higher temperature, inasmuch as it cannot, so long as it is free to evaporate, be raised to a temperature beyond the boiling-point, it will, when boiling, take readily the extra heat from the furnace and superheated steam, and the rod p, immersed in it, will in turn absorb it from the liquid, which thus conveys it to the rod,causing the latter by its consequent expansion to control the valve F to reduce the temperature of the steam. v \Vhile 500 Fahrenheit is mentioned as the desired normal temperature to be maintained in the retort, it'ma be increased or diminished in accordance with particular requirement and by proper adjustment of the valve F in its'steam-chest F.

The hydrocarbon oil supplied to the receptacle I is introduced into the retort with a jet of steam,which effects the introduction in a thoroughly tagged condition of the oil, and at the same ime the oxygen introduced by the steam-jet through the pipe 9 and box it is brought into intimate contact with the sulphur contained in the oil at a temper?- ture favorable to chemical union therewith.

The presence of a body of steam in the retort prevents therein any sudden increase of temperature as might otherwise be produced by the chemical union of the sulphur and oxygen.

All that portion of the injected hydrocarbon oil which boils at and below 500 Fahrenheit is converted by the action described into vapor, which passes off through the conduit (1 into the condenser. The residuum of distillation (a tar-like substance) accumulates at the bottom of the retort, whence it may be drawn off from time to time through the pipe q, and the sulphurous-oxide gas passes into the condenser with the distillate, from which it may be readily separated in any suitable or well-known manner.

The purpose of the pressure-regulating valve L is to produce uniform pressure in the boxes 7t and 715', and the provision of an overflow from the supply-receptacle I induces unvarying pressure on the valve 2" in the sup ply-pipe 11, the arrangement insuring the delivery into the retort of steam, hydrocarbon oil, and oxygen or other agent in unvarying quantities proportional according to requirement.

\Vhat I claim as new, and desire to secure by Letters Patent, is

1. The process of distilling and desulphurizing volatile hydrocarbon oils, which consists in heating a quantity of hydrocarbon oil of high specific gravity in a still, and injecting a lighter hydrocarbon oil into the still with steam and oxygen, the steam being alternately superheated or wet, according to the temperature of the bath, substantially as and for the purpose described.

2. In an apparatus for distillingand desulphurizing hydrocarbon oil, the combination of a retort A, a suitable fire-chamber, a superheater G, communicating witha steam-generator, a thermostat D in the retort, a steamchest F, communicating with the steam-gener- ITO ator and superheater and with the retort A, a valve F in the steam-chest and connected With and controlled by the thermostat, and an oil-supply pipe and an oxygen-supply pipe, both leading into the retort With the steamsupply, substantially as described.

3. In an apparatus for distilling and desulphurizing hydrocarbon oil, the combination of a retort A, having chambers k and it leading into it, and communicating, respectively, with the oil-supply pipe and the supply-pipe of oxygen, a fire-chamber 1, containing a superheater G, communicating With a steamgenerator, a thermostat D -in the retort, a steam-chest F, communicating from one side with the steam-generator and superheater and from its opposite side with the retort at the chambers 71; and 76 and a valve F in the steam-chest connected with and controlled by the thermostat, substantially as described.

4. In an apparatus for distilling and desulphu rizing hydrocarbon oil, the combination of a retort A, having chambers 713 and k leading into it, and communicating, respectively, with the oil-supply pipe and the supply-pipe of oxygen, a fire-chamber 0", containing a superheater G, communicating with a steam-generator E, athermostat D, comprising a metal rod 13 Within a tube 13, supported in the retort, a steanrchest F, communicating from one side With the steam-generator and superheater and from its opposite side with the retort at the chambers 7s and 7a,,a pressureregulator L in the communication of the steam-chest with the retort, a piston-valve F in the steam-chest F, and a lever 11, connecting the piston-valve with the rod 9, substantially as described.

5. In an apparatus for distilling and desulphurizing hydrocarbon oil, the combination, with a condenser O, boiler E, and oil--receptacle I, of a retort A, having chambers k and 7t leading into it, and communicating, respectively, With the receptacle I and the supply-pipe of oxygen, a fire-chamber '1', containing a superheater G, communicating with the boiler E, a thermostat D in the retort, a steam-chest F, having ports a: and a in one side and ports 9: and 00 in'its opposite side, and communicating at the ports 00 and a2, respectively, with the boiler and superheater, a valve F in the steam-chest, connected with and controlled by the thermostat, a pipe 1, communicating at one end with the steam-chest at the ports 50 and x and leading into the chamber is, a pressure-regulator L in the pipe 1, a branch pipe h, leading from the pipe Z into the chamber 7;, an overflow for the receptacle I, and a tar-pipe q, leading from the retort, the whole being constructed and arranged to operate substantially as described.

'* FRANK V. MINSHALL.

In presence of JULIA MINsHALL, THOMAS EWART. 

